REACTIONS OF TRICHLOROPHOSPHAZO-N-SULFURYLCHLORIDE AND ITS DERIVATIVES I - SYNTHESIS OF A NEW HETEROCYCLE CONTAINING P, N, S, AND C ATOMS IN ITS 6-MEMBERED RING - CRYSTAL-STRUCTURES OF (CH3)(3)SIN(H)P(CL-2) NS(O-2)CL, (CH3)(3)SIN(CH3)P(CL-2)NS(O-2)CL, AND P(CL-2)NS(O-2)N(H)C(CH3)N AT 150 K

Trichlorophosphazo-N-sulfurylchloride Cl3PNS(O-2)-Cl (1) reacts with [ (CH3)(3)Si](2)NR, R = H, CH3 to give its N-trimethylsilyl derivatives (CH3)(3)SiN(H)P(Cl-2)NS(O-2)Cl (2) and (CH3)(3)SiN(CH3)P(Cl-2) NS(O-2) Cl (3). At elevated temperatures (2) reacts with CH3CN under an intram olecular elimination of (CH3)(3)SiCl and a formation of 3,3-dichloro-5 -methyl-6H-1,2,4,6, 3-thiatriazaphosphinine-1,1-dioxide P(Cl-2)NS(O-2) N(H)C(CH3)N. All compounds were characterized by their 3;P-NMR spectra and chemical analysis and their identity was established by their cry stal structure determination. (2): Orthorhombic, S.G. P2(1)2(1)2(1), w ith a = 9.425(2), b = 10.507(3), c = 12.803(5) Angstrom, D-x = 1.591 g /cm(3), Z = 4, reflections collected 1796, final R = 0.0392; (3): Orth orhombic, S.G.P2(1)2(1)2(1), with a = 6.275(2), b = 12.638 (3), c = 16 .759(7) Angstrom, D-x, = 1.587 g/cm(3), Z = 4, reflections collected 1 816, final R = 0.0370; (4): Orthorhombic, S.G. Pna2(1),, with a = 7.78 4 (2), b = 13.911(3), c = 7.413(1) Angstrom, D-x, = 1.953 g/cm(3),Z = 4, reflections collected 2558, final R = 0.0265.